International Journal of Advanced Engineering Research and

Science (IJAERS)
ISSN: 2349-6495(P) | 2456-1908(O)
Vol-8, Issue-3; Mar, 2021
Journal Home Page Available: https://ijaers.com/
Journal DOI: 10.22161/ijaers
Article DOI: https://dx.doi.org/10.22161/ijaers.83.2

Production and characterization of caffeic acid-loaded

microfibrous polycaprolactone mats obtained by
electrospinning technology
João de Deus Pereira de Moraes Segundo1*, Maria Oneide Silva de Moraes2, Ana Lorena
de Brito Soares3, Gedeandro Gonçalves dos Santos4, Rudyere Nascimento Silva5,
Rosemeire dos Santos Almeida6,7,8, Walter Ricardo Brito9, Marcos Akira d’Ávila1

1Department of Manufacturing and Materials Engineering, University of Campinas, Brazil

2Thematic Laboratory of Microscopy and Nanotechnology, National Institute of Amazonian Research, Brazil
3Department of Chemical Engineering, Federal University of Ceará, Brazil
4General coordination of monitoring industrial projects, Superintendency of the Manaus Free Trade Zone, Amazonas, Brazil
5Department of Chemistry, Environment and Food, Federal Institute of Education, Science and Technology of the Amazonas, Brazil
6Department of Mechanical Manufacturing, Faculty of Technology Mauá, Brazil

7Department of Industrial Production Management, Faculty of Technology Luigi Papaiz, Brazil

8Department of Advanced Manufacturing, Faculty of Technology Adib Moisés Dib, Brazil
9Department of Chemistry, Federal University of Amazonas, Brazil

*Email: joaomoraessegundo@gmail.com

Received: 28 Nov 2020; Abstract— Microfibrous polycaprolactone (PCL) mats containing caffeic
Received in revised form: acid were manufactured by electrospinning technology. Electrospun PCL
fibers were processed with different concentration of caffeic acid, such as
03 Feb 2021;
0.10, 0.25, 0.50, and 1.00% in mass (m/m). The morphologies were
Accepted: 15 Feb 2021; observed by scanning electron microscopy (SEM). All produced fibers
Available online: 05 Mar 2021 exhibited random direction and different values of diameters. The caffeic
acid did not significantly affect the diameters of the PCL fibers in terms of
©2021 The Author(s). Published by AI
mean±SD, but some compound concentrations caused the anomaly
Publication. This is an open access article
formation in the electrospun fibers' structure, with the exception of 0.10%
under the CC BY license
CA. Wettability tests in the microfibrous PCL mat with or without caffeic
(https://creativecommons.org/licenses/by/4.0/).
acid showed hydrophobic behavior due to air effect, same with the caffeic
Keywords—Polycaprolactone, caffeic acid amount increase. On the other hand, contact angle measurements
acid, electrospun microfibrous mat, decrease with the caffeic acid amount increase. The same occurred with
electrospinning. the caffeic acid-loaded PCL films. The chemical characterization by FTIR
showed the influence of the concentrations of CA in the PCL microfibers,
indicating the presence of hydrogen bonds, with the exception of 1.00%
CA. We suggest that the 0.10% caffeic acid concentration is the most
suitable, mainly due to the absence of anomalies on the surface of the PCL
microfibers for future investigations, such as antimicrobial and
cytotoxicity tests, drug release, etc.

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João de Deus Pereira de Moraes Segundo et al. International Journal of Advanced Engineering Research and Science, 8(3)-2021

I. INTRODUCTION fiber PCL diameters was due to the use of H2O as an

Electrospinning is widely used to produce fibers, additive in the PCL solution in glacial acetic acid that
generally of a polymeric nature [1]. These electrospun increased the electrical conductivity due to the acetic acid
fibers are obtained from a polymer solution or polymer ionization.
melt [2]. The technique is low cost and easy to implement The versatility of the electrospinning technology
when compared to other fiber manufacture methods [3]. allows the production of electrospun fibers containing
Moreover, other techniques, i.e., dual syringe [4], coaxial others material types [1], i.e., polymer nanoparticles [25],
[5], melt [6], and multiple needle electrospinning [7], are metallic or ceramic nanoparticles [1], drugs [1,3], oils [2],
derivations of traditional electrospinning. For this reason, and bioactive compounds [27].
electrospinning technology has been used extensively in Caffeic acid is a phenolic compound from vegetables
manufacturing fibers that can acquire nanometric widely used in pharmacological and cosmetic areas. It is
dimensions [1-3]. an excellent antioxidant used to prevent premature aging;
The electrospun fibers during their processing are it has antimicrobial activity and is even capable of acting
deposited on a grounded metallic collector [8]. After this as a cancer inhibitor [28].
continuous deposition, a fibrous mat is formed with Electrospinning has been used to manufacture caffeic
typically porous, light weight, and flexible characteristics acid-based biodegradable polymer fibers [29-31]. These
[8,9]. Other denominations for the fibrous mats obtained electrospun fibrous mats presented potential biomedical
via electrospinning are found in the literature, i.e., and packaging applications.
nanofibrous membrane [10], membrane [11,12], nonwoven
This work aims to show the production and
mat [13], -nano and -microfibrous mats [14,15].
characterization of PCL fibers containing caffeic acid to
The applications of electrospun fibers are diverse and define the suitable concentration of phenolic compound in
include the sensors [16], biosensors [17], filtration [18], electrospun fibers.
purification [19], biomedical [20], and pharmaceutical
fields [21].
II. EXPERIMENTAL
Concerning the biomedical field, electrospun fibers
have achieved prominence in the controlled release of 1.1 Materials
drugs, which are delivery devices that generally combine Were used poly(caprolactone) (PCL, MM=80,000
biodegradable and biocompatible polymers with drugs [19- g/mol) and caffeic acid (CA, MW=180.16 g/mol)
22]. And in the production of scaffolds for cell purchased from Sigma-Aldrich. The solvents chloroform
proliferation aiming application in tissue engineering [22]. and acetone were purchased from Labsynth. Potassium
The most widely used biodegradable and bromide (KBr, MW=119.00 g/mol) purchased from
biocompatible polymers in the biomedical field are poly Merck. Deionized water with electrical conductivity of 0.5
(glycolic acid) (PGA), poly (L-lactic acid) (PLLA), poly μS/cm2 was used.
(lactic-co-glycolic acid) (PLGA), poly (L-lactide) (PLA), 1.2 Prepare of the solutions
poly (D-lactic acid) (PDLA), and poly (ε-caprolactone)
The PCL solution was prepared by mixing chloroform
(PCL) [22,23].
(3.16 g) and acetone (3.16 g) into a glass flask under
PCL is a biodegradable polymer of synthetic source, mechanical stirring for 15 minutes. Posteriorly, 1g of PCL
aliphatic polyester and semicrystalline, has interesting was added to the solvent mixture for dissolution, which
properties, such as good mechanical properties, is lasted 24 hours.
biocompatible, and non-toxic [23,24]. PCL is soluble in
Caffeic acid was only used after preparing the PCL
organic solvents and is considered a polymer excellent to
solution, and different amounts of the compounds given
produce PCL fibers by electrospinning [24,25].
percent by mass, such as 0.10, 0.25, and 0.50% CA, were
Electrospun PCL fibers with diameters of 1.660 ± added to the solution under mechanical stirring for 4 hours
1.120 µm were prepared using chloroform and acetone as until its complete dispersion.
solvents. The PCL fibers of micrometric scale exhibited a
1.3 Prepare of the PCL fibers loaded with caffeic acid
smooth surface in their morphology shown by SEM image
[25]. Nevertheless, Li et al. [26] produced PCL fibers of In order to prepare the caffeic acid-loaded PCL fibers,
nanometric diameters around 200±78 nm with a diameter the PCL solution containing the caffeic acid was placed
maximum of 613 nm and diameter minimum of 97 nm. into the syringe with a metallic needle of diameter Øneedle =
The authors reported that this optimization to reduce the 0.8mm. After that, conducted to the electrospinning, which

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João de Deus Pereira de Moraes Segundo et al. International Journal of Advanced Engineering Research and Science, 8(3)-2021

was parameterized with flow rate of Q=8mL/h, applied resolution) at room temperature. ImageJ software (version
tension of V=14 kV, and work distance of dw=180 mm. free) obtained the contact angle measurements (in
The electrospun fibers were manufactured on the grounded triplicate) using the Low Shape Axisymmetric Drop Shape
metal rectangular collector at temperature of T = 22.0±0.5 Analysis tool. Casting films with and without CA were
°C and relative humidity of RH = 57.0±1.0 %. Fig. 1 prepared for comparative study.
shows a schematic illustration of the experimental setup
this work.
III. RESULTS AND DISCUSS
Fig. 2 shows the SEM images of the PCL fibers with
500X magnitude and 20 µm scale (a), 1,000X magnitude
and 10 µm scale (b), 5,000X magnitude and 2 µm scale
(c). They reveal the morphological characteristic of the
electrospun fibers that exhibited random direction. This
effect is typical in electrospun fibers produced with a static
rectangular metallic collector [32]. Fibers with different
diameters were observed. About this, the main
disadvantage of electrospinning technology is no guarantee
of equal diameters for all electrospun fibers [33], which
was expected.
Fig. 1: Schematic illustration showing basic In Fig. 2c is presented the surface morphology of the
electrospinning items and the PCL solution with CA. PCL fibers, showing the rough surface of the fibers. This
surface morphological characteristic for electrospun PCL
1.4 Morphological characterization
fibers occurs due to the solvent nature used [34] or the
The morphology of the electrospun PCL fibers and effect of the humidity [35]. On the other hand, it is more
caffeic acid-loaded PCL fibers was observed by Scanning common to observe smooth surface morphology in
electron microscopy – SEM (ZEISS, Evo MA-15 model). electrospun PCL fibers, as reported Moraes Segundo et al.
Before analyzing the samples in SEM, they were coated [25] that obtained PCL fibers of smooth surface.
with gold sputtering (BAL-TEC, SCD 050 model).
The Fig. 2d – 2p are shown the morphology of the
1.5 Measurements and Statistical analysis of fiber caffeic acid-loaded PCL fibers with different amounts of
diameters the compound. All the SEM images showed that the
ImageJ software (free version) was used to measure the electrospun fibers remained in random direction.
fiber diameters from SEM images of 1,000X magnitude. In particular, the PCL fibers with 0.10% CA did not
The average values and standard deviations (average ± present anomaly in their structure (see Fig. 2d and 2e),
S.D.), minimum diameter (Dmin), and maximum diameter whereas the Fig. 2f shows the caffeic acid existence in the
(Dmax) were represented based on methods described in the fibers.
literature [25].
PCL fibers produced with 0.25% CA showed that the
1.6 Chemical Characterization amount of caffeic acid used to bring on an excess of the
Chemical characterization was performed by infrared compound out of electrospun fibers can be seen by SEM
spectroscopy – IR. Samples were mixed with potassium images in Fig. 2g and 2h. Moreover, the presence of
bromide (KBr) in 1:100 and pressed to 2.5kN for 5 precipitated caffeic acid was observed and is showed in
minutes to produce tablets with 15 mm diameter Fig. 2i. However, this concentration did not cause the
containing the samples. After that, they were analyzed in formation of anomalies in the fiber structure. Differently
the spectrometer (Thermo Scientific – NICOLET iS5, for the concentrations of 0.50 and 1.00% CA, the anomaly
model) in the 400 – 4000 cm-1 range, 16 scans with a formation and CA precipitation were observed, as shown
spectral resolution of 4cm-1. in SEM images of Fig. 2j – 2m and Fig. 2n – 2p,
respectively.
1.7 Wettability and Contact angle measurements by
ImageJ software Electrospun PCL fibers presented diameters of 2.50 ±
1.12 µm, Dmin = 0.48 µm, and Dmax = 4.60 µm. These
The wettability test was performed using water, where
values on the structural dimensions of the micrometric-
on the surface of the sample was placed a 10 µL drop
sized fibers explain the name given to the nonwoven mat,
using a pipette. The water drop was observed with a digital
like a microfibrous PCL mat.
microscope (TQC – Lite plus model, with 1.000X

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João de Deus Pereira de Moraes Segundo et al. International Journal of Advanced Engineering Research and Science, 8(3)-2021

Fig. 2: SEM images of the PCL microfibrous mat (a – c), and with 0.10 % CA (d – f), 0.25% CA (g – i), 0.50% CA (j – m),
and 1.00% CA (n – p), showing the morphologies of the fibers produced by electrospinning.

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João de Deus Pereira de Moraes Segundo et al. International Journal of Advanced Engineering Research and Science, 8(3)-2021

Fig. 6: Comparative FTIR spectra of caffeic acid, PCL fibers, and caffeic acid-loaded PCL fibers (a). FTIR spectra of PCL
fibers without and with caffeic acid of 0.10%, 0.25%, 0.50%, 1.00% CA (b).

The diameter values of the PCL fibers with and without application studies, i.e., antimicrobial tests, cytotoxicity
caffeic acid are listed in the Table 1. The results showed tests, drug release, etc.
that we did not obtain nanometric size fibers to any
a) 5 b) 15
concentration of caffeic acid used. Furthermore, the caffeic

fiber diameters maximum

acid did not significantly change the fiber diameters that 4
fiber diameters

Electrospun
Electrospun

10
were expressed in mean ± S.D. In the graph presented in 3

(m)
(m)

Fig. 3a show this effect. 2

5

Table.1: Structural measurements of the microfibers 1

obtained from SEM images. 0 0

10 L

25 A

50 A

00 A

A
PC
10 L

25 A

50 A

00 A

C
PC

%
Diameters Dmin Dmax
%

0.

0.

0.

1.
Microfibrous
0.

0.

0.

1.

PCL fibers with and without

(mean±SD) (µm) (µm) PCL fibers with and without
caffeic acid
caffeic acid
PCL 2.50±1.12 0.48 4.60
PCL + 0.10% CA 2.03±1.05 0.25 4.94 Fig. 3: Graphs of the fiber diameters expressed in mean ±
S.D (a) and Dmax (b) with and without CA.
PCL + 0.25% CA 2.40±0.95 0.40 5.15
PCL + 0.50% CA 1.96±1.40 0.45 8.20
Fig. 4 presents the graph of the contact angle
PCL + 1.00% CA 2.41±1.53 0.33 10.23 measurements of the microfibrous mats and films with
CA = caffeic acid different CA concentrations. Contact angle when higher
than 90° classifies a surface as hydrophobic and less than
90° as hydrophilic, using the water as solvent [36].
Under other conditions, the Fig. 3b present the graph
All microfibrous mats with or without CA showed
considering the mean and maximum (Dmax) values of the
contact angle greater than 90°, differently for the films
fiber diameters containing caffeic acid. Then, we observed
that the presence of fibers with larger diameters is related with or without CA that exhibited contact angle less than
to the addition of caffeic acid. 90°, as shown in Fig. 4, which shows the influence of the
presence of air in the electrospun mats due to its porosity
Briefly on incorporating caffeic acid, small amounts of that forms air pockets [37].
CA were incorporated successfully in PCL fibers by
electrospinning technology. However, we suggest the PCL is considered relatively hydrophobic [38,39],
concentration of 0.10% CA, which did not present which may be related to the hydrophilic carbonyl groups
present in its structure. The PCL film had a contact angle
anomalies in its structure and did not influence the
of 79.88° ± 3.25° (less than 90°), corroborating with the
diameter of the fibers, being the most suitable for future
literature [40].

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João de Deus Pereira de Moraes Segundo et al. International Journal of Advanced Engineering Research and Science, 8(3)-2021

Contact angle measurements also examined PCL films cm-1; and the aromatic C=C stretching present in the
containing caffeic acid and cast films with concentrations aromatic ring at 1445 cm-1 [41-43].
of 0.10, 0.25, 0.50, and 1.00% CA that exhibited a contact For the PCL, the most relevant vibrational bands were
angle of 78.11° ± 6.02°, 77.04° ± 11.83°, 72.04° ± 5.93°, determined, the asymmetric and symmetrical double of
and 72.41° ± 2.65°, respectively. High S.D. values may CH2 at 2952 cm-1 and 2873 cm-1, respectively; the
indicate a heterogeneous and aggregated distribution of carbonyl C=O stretching of the ketone group at 1735 cm-1;
CA on the surface of the PCL film. and the –OH stretching of water adsorbed at 3449 cm -
1
150 [44,45].
a) 100
measurements ()

120
Contact angle

measurements ()
 = 90 90

Contact angle
90

60 80

LEGEND:
30 70
microfibrous mats
film
0
60
0.00 0.25 0.50 0.75 1.00 1.25
0.0 0.5 1.0
Caffeic acid concentration Caffeic acid concentration
(%m/m) (%m/m)
Fig. 4: Graph of the contact angle measurements versus b) 150
different CA concentrations.
measurements ()

140
Contact angle

The contact angle for microfibrous PCL mats indicated

130
a hydrophobicity because the contact angle was of 136.32°
± 7.84° (higher than 90°). In Fig. 5b is shown the graph of
120
the contact angle for microfibrous PCL mats with CA
concentrations (0.10, 0.25, 0.50, and 1.00%), where was 110
decreased to 123.44° ± 1.06°, 121.81° ± 3.23°, 129.08° ± 0.0 0.5 1.0
0.43°, and 120.96° ± 3.65°, respectively (see the red Caffeic acid concentration
dashed line in Fig 5b), indicating the influence of CA in (%m/m)
reduce the hydrophobicity of microfibrous PCL. In Fig. Fig. 5: Graph of the contact angle measurements versus
6b, a red dashed line shows the changes caused by the different CA concentrations of the (a) films and (b)
presence of CA, mainly for the concentration of 0.10% of microfibrous mats.
CA that presented less variation in the contact angle,
therefore, showing a better distribution of CA on the
surface of the PCL fibers. Note that in the FTIR spectrum for the caffeic acid-
The chemical characterization was performed using loaded PCL fibers (red curve), there is a strong decrease in
infrared spectroscopy to determine the vibrational modes the intensity of the vibrational modes in the fingerprint
present in the polymeric matrices obtained before and after region (1800 - 700 cm-1) referring to the polymeric matrix
the addition of the antioxidant caffeic acid. of caprolactone indicating that the caffeic acid interacts
strongly with the PCL polymer chains. In the vibrational
Fig. 6a shows three FTIR spectra corresponding to caffeic region of the carbonyl (green region), the presence of two
acid, caffeic acid-loaded PCL fibers and PCL fibers different types of carbonyl inherited from the ketone group
comparatively. of the PCL and the carboxylic acid of the caffeic acid is
For caffeic acid, the main vibrational bands were observed.
identified, the –OH stretching from adsorbed water and After the gradual addition of CA, we observed the
hydroxyls present in the molecule at 3428 cm -1 and 3233 chemical influence of CA in the PCL matrix. Fig. 6b
cm-1, respectively; the –CH stretching at 2981 cm-1; the shows the chemical influence of the progressive presence
carbonyl C=O stretching of the carboxylic acid at 1643 of the CA molecule in the polymeric matrix of the PCL.
The increase in the concentration of CA reflects the

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João de Deus Pereira de Moraes Segundo et al. International Journal of Advanced Engineering Research and Science, 8(3)-2021

decrease in the transmittance of the vibrational bands of The authors would like to thank Amazonas State
the PCL. Research Support Foundation – FAPEAM (proc.
However, there is a limit. In concentrations below 062.00113/2016), SisNANO Program, MCTIC, CNPq for
1.00% CA, there is only interference in the transmittance financial support.
of the vibrational modes, i.e., the intensity of the
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